CN107917904B - Rapid detection Fe3+Method (2) - Google Patents

Rapid detection Fe3+Method (2) Download PDF

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CN107917904B
CN107917904B CN201711140355.0A CN201711140355A CN107917904B CN 107917904 B CN107917904 B CN 107917904B CN 201711140355 A CN201711140355 A CN 201711140355A CN 107917904 B CN107917904 B CN 107917904B
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王灯旭
孙瑞雪
冯圣玉
刘鸿志
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Shandong University
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N2021/6432—Quenching

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Abstract

The invention relates to a blockRapid detection of Fe3+Method of using Fe3+Detection of Fe in solid or solution with test paper3+Trace detection of (1), Fe3+Detecting the minimum concentration of 10‑7mol/L of said Fe3+The detection test paper is made of filter paper loaded with fluorescent material, and is Fe3+After the test paper is repeatedly used for 2 times, the fluorescence intensity can keep more than 90% of the initial intensity, and after the test paper is repeatedly used for 10 times, the fluorescence intensity can still keep more than 75% of the initial fluorescence intensity. The detection method of the invention has the advantages of accuracy, rapidness, high sensitivity and Fe tolerance3+Has strong selectivity, can eliminate the interference of other metal ions, and uses Fe3+The fluorescent material loaded by the test paper is insoluble in a water phase or an organic phase, the fluorescence intensity and sensitivity of the test paper are kept unchanged in the detection process, and trace detection can be carried out.

Description

Rapid detection Fe3+Method (2)
Technical Field
The invention relates to a method for rapidly detecting Fe3+Belonging to the technical field of metal ion detection.
Background
Iron ion (Fe)3+) Is a ubiquitous metal ion in cells and plays a crucial role in various cell functions. Because iron ions are easy to undergo redox reaction and have strong affinity with oxygen elements, iron ions play an important role in DNA and RNA metabolism and electron transfer processes. The transport and storage of large amounts of iron ions present in the body is closely linked to the transport and storage of various enzymes and specific proteins, and small amounts of Fe are also present in organic anions (phosphates and carboxylates), multiple ligands (i.e. to generate chelates, polypeptides), cell membrane surface compositions or extracellular matrices (glycans and sulfonates)3+. Normally, the liver stores and fixes a large amount of iron element, for example, the excessive deposition of iron in the liver may cause hepatocyte damage and liver fibrosis, participate in carcinogenesis through 3 mechanisms such as oxidative stress induction, tumor growth promotion and immune system modification, and may cause serious complications. Research on iron ions has attracted research interest due to their important role in biological systems and the environment. How to qualitatively or quantitatively determine the concentration of iron ions in clinic,Has important research significance in medical, environmental and other industrial samples.
There are many detection methods for detecting iron ions, such as inductively coupled plasma mass spectrometry (ICP-MS), atomic absorption spectrometry, voltammetry, electrochemistry, colorimetry, flame photometry, and fluorescence. Among these methods, the fluorescence method is attracting attention due to its outstanding advantages, and has the advantages of high sensitivity, good stability, etc. However, the conventional fluorescence detection method uses expensive fluorescence detector, is inconvenient to carry, and cannot eliminate copper ions (Cu)2+) And cobalt ion (Co)2+) Interference of plasma, therefore in Fe3+The rapid qualitative detection aspect of the method shows obvious disadvantages. And the conventional fluorescent materials for the fluorescent test paper are all soluble (see: Biosensors and Bioelectronics,2017,99,303-311.), but these test papers based on the soluble fluorescent materials detect Fe in the aqueous phase or the organic phase3+In this case, the material is easily dissolved in the aqueous phase or the organic phase, and the fluorescence intensity of the test paper itself is reduced due to the loss or dilution of the material, thereby decreasing the sensitivity of the test paper.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for rapidly detecting Fe3+The method of (1), which can detect Fe in an aqueous phase, an organic phase or a solid3+The interference of other metal ions is eliminated in the detection process, the limitation of the traditional metal ion detection is overcome, and the method can be used for detecting Fe3+Has strong selectivity, improves the detection sensitivity, has quick and sensitive detection method, and uses Fe3+The detection test paper has good reusability.
The technical scheme of the invention is as follows:
rapid detection Fe3+Method of using Fe3+Detecting Fe in solid or solution with test paper3+Trace detection of (1), Fe3+Detecting the minimum concentration of 10-7mol/L of said Fe3+The detection test paper is made by loading a fluorescent material on filter paper, the fluorescent material is a polyhedral silsesquioxane-based fluorescent porous material, and Fe3+After the test paper is repeatedly used for 2 times, the fluorescence intensity can keep more than 90% of the initial intensity, and after the test paper is repeatedly used for 10 times, the fluorescence intensity can still keep more than 75% of the initial fluorescence intensity.
According to the invention, Fe is preferably detected rapidly3+The method comprises the following steps:
examination of Fe3+Detecting whether the test paper is effective;
using Fe3+Detecting the detected object by using detection test paper;
mixing Fe3+Dissolving and detecting the test paper.
According to the invention, preferably, said test Fe3+The steps for detecting whether the test paper is effective are as follows: mixing Fe3+The test paper is placed under ultraviolet light to observe whether the test paper emits fluorescence or not, and the test paper emits visible obvious fluorescence under the ultraviolet light, so that the test paper is effective and can be directly detected.
According to the invention, preferably, said use of Fe3+The step of detecting the detected object by the detection test paper is as follows: fe to be measured3+Solution or solid with Fe3+The detection test paper is contacted, kept stand for 10-20 seconds at room temperature, and Fe is taken out3+Test paper for Fe3+After the test paper is dried, the test paper is placed under ultraviolet light to observe the fluorescence change of the test paper by naked eyes, and if the test paper generates a fluorescence quenching phenomenon, the Fe contained in the sample is judged3+If the test paper has no fluorescence quenching phenomenon, the sample is judged to contain no Fe3+。
Further preferably, Fe to be measured3+The contact mode of the solution and the fluorescent test paper is as follows: dripping the solution to be detected on the test paper, or immersing the test paper in the solution to be detected; fe3+The contact mode of the solid and the fluorescent test paper is as follows: the solid powder or particles are applied to a test strip.
According to the invention, preferably, the Fe3+Dissolving, and the detection test paper recovery step is as follows: will be detected with Fe3+The test paper is put into a pure solvent to be soaked to lead Fe3+Dissolving in solvent, taking out the test paper, drying, observing under ultraviolet lamp, recovering fluorescence of the fluorescent test paper, and performing next detection.
Further preferably, the detected Fe3+And soaking the test paper in a pure solvent for 1-10 min.
Further preferably, the pure solvent is dissolved Fe3+The solvent of (3) is selected from one of water, methanol, ethanol, dichloromethane, chloroform or acetone.
Preferably, according to the invention, the wavelength of the ultraviolet light is 365 nm.
Preferred according to the invention, Fe3+The test paper is prepared by the following method:
(1) fully grinding the fluorescent porous material, adding a solvent as a dispersing agent, performing ultrasonic dispersion uniformly to obtain a suspension, loading the fluorescent material on filter paper, and naturally drying;
(2) soaking the test paper in a soaking solvent, removing redundant fluorescent porous material powder on the surface of the filter paper, taking out the filter paper, naturally drying, and shearing into test paper strips to obtain Fe3+And (5) detecting test paper.
According to the invention, the fluorescent porous material in the step (1) is preferably a polyhedral silsesquioxane-based fluorescent porous material, the polyhedral silsesquioxane-based fluorescent porous material is a fluorescent porous polymer prepared by Heck reaction of octavinyl silsesquioxane (OVS) and halogenated aromatic compound, and the Brunauer-Emmett-Teller (BET) specific surface area is 200-2000 m2g-1Pore volume of 0.4-1.5 cm3g-1。
Reaction of octavinyl silsesquioxane (OVS) with a halogenated aromatic compound is as follows:
Figure BDA0001471345090000031
x＝Br，I
preferably, in the step (1), the loading amount of the fluorescent material is 0.5-0.8 mg/cm2Most preferably, the loading of the fluorescent material is 0.6mg/cm2。
According to the present invention, in the step (1), the dispersing solvent is one or a mixture of any two or more selected from ethanol, methanol, tetrahydrofuran, dichloromethane, chloroform and acetone.
Preferably, in step (1), the molar volume ratio of the fluorescent material to the dispersant is: 0.3-0.8: 1 mg/mL.
According to the invention, in the step (1), the ultrasonic dispersion time is preferably 0.5-2 h.
Preferably, in step (1), the loading manner of the fluorescent material on the filter paper is as follows: and (3) uniformly immobilizing a layer of fluorescent material on the surface of the filter paper through vacuum filtration, and continuing the filtration for 1-2 min.
Preferably, in step (2), the soaking solvent is one or more selected from ethanol, methanol, tetrahydrofuran, dichloromethane, chloroform and acetone.
According to the invention, in the step (2), the soaking time is preferably 1-10 min.
Fe3+The detection mechanism of the detection test paper is as follows: the fluorescent porous material is synthesized through Heck crosslinking reaction of cage POSS and halogenated aromatic compound, and the introduction of the cage POSS structure inhibits the aggregation of the fluorescent material so as to improve the luminous efficiency of the material. In addition, the porous structure of the material can further improve the luminous intensity of the fluorescent material. As the cage-shaped POSS is an organic-inorganic hybrid framework material with stable and rigid structure, POSS molecules can be connected by a plurality of covalent bonds to form a cross-linked structure through Heck reaction, and the formed porous material is insoluble in a water phase and an organic phase. When the polymer containing the cross-linked structure interacts with a detected substance in the detection process, the generated charges and energy can be effectively transferred along the conjugated molecular chain, and the effect is multiplied, so that the detection sensitivity is effectively improved, and the detection method is more superior to the corresponding small-molecule fluorescent compound. When Fe is present in the system3+When present, due to Fe3+The fluorescent material cannot absorb ultraviolet light due to absorption of the ultraviolet light, so that the fluorescent material cannot be excited to generate fluorescence, and a fluorescence quenching phenomenon which can be observed by naked eyes is caused. Since the fluorescent porous material is insoluble in water and organic solvents, and Fe3+Is easy to dissolve in water and organic solvent,therefore, the used fluorescence detection test paper can be soaked in water or pure solvent to remove the residual Fe on the test paper3+Dissolving, so that the fluorescence property of the test paper is recovered, and Fe can be repeatedly carried out3+And (6) detecting.
The invention has the following beneficial effects:
1. the detection method of the invention has the advantages of accuracy, rapidness, high sensitivity and Fe tolerance3+Has strong selectivity (shown in figure 1), can eliminate the interference of other metal ions, and uses Fe3+The fluorescent material loaded by the detection test paper is insoluble in a water phase or an organic phase, the fluorescence intensity and sensitivity of the test paper are kept unchanged in the detection process, trace detection can be carried out, and Fe3+Detecting the minimum concentration of 10-7mol/L。
2. Fe used in the detection method of the present invention3+After the detection test paper is repeatedly used for 2 times, the fluorescence intensity can keep more than 90% of the initial intensity, and after the detection test paper is repeatedly used for 10 times, the fluorescence intensity can still keep more than 75% of the initial intensity, so that the detection test paper has excellent reusability. The raw materials are easy to obtain, the preparation method is simple and convenient, and the loaded fluorescent material is insoluble in a water phase or an organic phase and is used as a fluorescent indicator, so that the influence of weakening the fluorescence intensity of the test paper caused by dilution of the fluorescent material by a solvent is avoided.
3. The detection method of the invention has high detection speed and can detect Fe to be detected3+Solution or solid with Fe3+The detection test paper is contacted, standing is carried out for 10-20 seconds at room temperature, and after the test paper is dried in the air, an obvious macroscopic fluorescence quenching phenomenon is generated immediately by observation under ultraviolet light.
4. The detection method is low in cost, visual, free of complex instruments and equipment and capable of carrying out on-site real-time naked eye quick detection only by one portable ultraviolet lamp.
5. Fe used in the detection method of the present invention3+The test paper has good reusability, and the used test paper can be repeatedly detected after being washed by water or an organic solvent, so that the production cost is further saved.
Drawings
FIG. 1 shows the concentrationsThe same concentration (1X 10) was added to a suspension of HPP-6 at 0.1mg/mL-3mol/L) of different metal ions. (formula for calculating quenching constant: I0/I＝1+KSV[M]In which I0Initial fluorescence intensity, I fluorescence intensity after quenching, KSVIs a fluorescence quenching constant, [ M ]]Is Fe3+And (4) concentration. )
FIG. 2 is a nitrogen adsorption and desorption curve of HPP-6 of the fluorescent porous material prepared in example 1.
FIG. 3 shows the fluorescence intensity and Fe of the test paper prepared in example 13+The concentrations are respectively 1 × 10-2mol/L、1×10- 3mol/L、 1×10-4mol/L、1×10-5mol/L、1×10-6mol/L、1×10-7Fluorescence response curves at mol/L and 0 mol/L.
FIG. 4 shows the test paper prepared in example 1 immersed in Fe3+A macroscopic fluorescence quenching phenomenon image occurs after the solution.
FIG. 5 is a graph showing the reusability of the test strips prepared in example 1. (Fe)3+The concentration is 1X 10-3mol/L, relative value calculated by taking the fluorescence intensity of the test paper used for the first time as 100%. )
FIG. 6 shows the fluorescence intensity and Fe of the test paper prepared in example 23+The concentrations are respectively 1 × 10-2mol/L、1×10- 3mol/L、 1×10-4mol/L、1×10-5mol/L、1×10-6mol/L、1×10-7Fluorescence response curves at mol/L and 0 mol/L.
FIG. 7 shows the test paper prepared in example 2 immersed in Fe3+A macroscopic fluorescence quenching phenomenon image occurs after the solution.
Detailed Description
The present invention will be further described, but not limited to, by the following specific embodiments in conjunction with the accompanying drawings.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
Rapid detection Fe3+The specific method comprises the following steps:
preparing a solution to be detected: preparing Fe with different concentrations3+Solution: fe3+The solution concentrations were: 1X 10-2mol/L、1×10-3mol/L、 1×10-4mol/L、1×10-5mol/L、1×10-6mol/L、1×10-7mol/L；
Further preferably, Fe to be measured3+The contact mode of the solution and the fluorescent test paper is as follows: dripping the solution to be detected on the test paper, or immersing the test paper in the solution to be detected; fe3+The contact mode of the solid and the fluorescent test paper is as follows: the solid powder or particles are applied to a test strip.
The detection method comprises the following steps: liquid detection: dropping the solution to be measured to Fe3+The method comprises the following steps of (1) carrying out fluorescence detection on a test strip, or immersing the test strip into solutions to be detected with different concentration gradients, taking out the test strip, and airing the test strip; solid detection: coating the solid powder or particles on a test paper; under the irradiation of 365nm ultraviolet lamp wavelength light, the test paper strip is used for detecting Fe with different concentrations3+The solution presents quenching phenomena of different degrees, thereby realizing the purpose of quenching Fe in sewage3+The qualitative detection of (2) is shown in fig. 3 and 4.
After the detection is finished, the test paper is soaked in 100mL of absolute ethyl alcohol for 4min, and Fe3+Dissolving the test paper in ethanol, recovering the fluorescence intensity of the test paper, and continuously using the test paper for the next detection; the reusability of the test strips is shown in figure 5.
Reusable Fe3+The fluorescent test strip is prepared by the following method:
(1) preparing a fluorescent porous material HPP-6:
octavinyl silsesquioxane (OVS) (633mg,1mmol) and catalyst Pd (OAc) under argon protection2(90mg,0.4mmol), cocatalyst P (o-CH)3Ph)3(193mg,0.94mmol), acid absorbent Et3N (15mL) was dissolved in dry N, N-dimethylformamide (45mL), magnetically stirred at room temperature for 0.5h, then 2,2',7,7' -tetrabromo-9, 9' -spirobifluorene (1.264g,2mmol) was added and reacted at 120 ℃ for 72 h.
And (3) post-treatment: suction filtering, washing with tetrahydrofuran, chloroform, water, methanol and acetone, Soxhlet extracting with tetrahydrofuran and methanol for 24 hr, and vacuum drying at 70 deg.C for 48 hr to obtain yellow solid. The yield was about 100%.
The synthesis route of octavinyl silsesquioxane (OVS) and 2,2',7,7' -tetrabromo-9, 9' -spirobifluorene for preparing fluorescent porous polymer is as follows:
Figure BDA0001471345090000061
HPP-6 was analyzed for specific surface area and porosity using a fully automatic specific surface area and micropore analyzer, and the nitrogen adsorption-desorption curve is shown in FIG. 2, with a BET specific surface area of 650m2g-1Pore volume of 0.53cm3g-1。
The fluorescence spectrophotometer is used for carrying out fluorescence analysis on HPP-6, the maximum fluorescence emission wavelength is 485nm, and green fluorescence is emitted under an ultraviolet lamp.
(2) Preparation of fluorescence detection test paper
Taking a certain amount of the fluorescent porous material HPP-6, uniformly grinding in a mortar, dispersing in absolute ethyl alcohol to prepare 40mL of 0.5mg/mL suspension, and ultrasonically dispersing for 30min to uniformly disperse; then putting the filter paper into the solution to enable Fe3+The fluorescent material is uniformly deposited on the filter paper, and is taken out and naturally dried; finally, the filter paper is cut into test strips with the length of 5cm and the width of 1 cm.
Example 2
Rapid detection Fe3+The specific method comprises the following steps:
preparing a solution to be detected: preparing Fe with different concentrations3+Solution: fe3+The solution concentrations were: 1X 10-2mol/L、1×10-3mol/L、 1×10-4mol/L、1×10-5mol/L、1×10-6mol/L、1×10-7mol/L；
The detection method comprises the following steps: mixing Fe3+The fluorescence detection test strip is respectively immersed in Fe with different concentration gradients3+In the solution, after the test strip is dried, the test strip is irradiated by ultraviolet light with the wavelength of 365nm, and the test strip is used for different concentrationsFe (b) of3+The solution presents quenching phenomena of different degrees, thereby realizing the purpose of quenching Fe in sewage3+The qualitative detection of (2) is shown in fig. 6 and 7.
After the detection is finished, the test paper is soaked in 100mL of absolute ethyl alcohol for 4min, and Fe3+Dissolving in ethanol, recovering the fluorescence intensity of the test paper, and continuously using for the next detection.
Reusable Fe3+The fluorescent test strip is prepared by the following method:
(1) preparing a fluorescent porous material HPP-1:
OVS (633mg,1mmol) was reacted with Pd (OAc) catalyst under argon blanket2(90mg,0.4mmol), cocatalyst P (o-CH)3Ph)3(193mg,0.94mmol), acid absorbent K2CO3(2.2g,16mmol) was dissolved in dry N, N-dimethylformamide (45mL), magnetically stirred at room temperature for 0.5h, then 4,4' -dibromobiphenyl (1.248g,2mmol) was added and reacted at 120 ℃ for 72 h.
And (3) post-treatment: filtering, washing with tetrahydrofuran, chloroform, water, methanol and acetone respectively, performing Soxhlet extraction with tetrahydrofuran and methanol respectively for 24h, and vacuum drying at 70 deg.C for 48h to obtain white solid. The yield was about 100%.
The method for preparing the fluorescence detection test paper by using the octavinyl polyhedral oligomeric silsesquioxane (OVS) and the 4,4' -dibromobiphenyl comprises the following synthetic route:
Figure BDA0001471345090000071
HPP-1 is analyzed for specific surface area and porosity by a full-automatic specific surface area and micropore analyzer, wherein the BET specific surface area is 592m2g-1Pore volume of 0.79cm3g-1。
The fluorescence analysis of HPP-1 is carried out by a fluorescence spectrophotometer, the maximum fluorescence emission wavelength is 428nm, and blue fluorescence is emitted under an ultraviolet lamp.
(2) Preparation of fluorescence detection test paper
Taking a certain amount of the fluorescent porous material HPP-1, uniformly grinding in a mortar, dispersing in absolute ethyl alcohol to prepare 40mL of 0.5mg/mL suspension, and ultrasonically dispersing for 30min to uniformly disperse; then putting the filter paper into the solution to enable the fluorescent material to be uniformly deposited on the filter paper, taking out and naturally drying; finally, the filter paper is cut into test strips with the length of 5cm and the width of 1 cm.

Claims (2)

1. Rapid detection Fe3+The specific method comprises the following steps:
preparing a solution to be detected: preparing Fe with different concentrations3+Solution: fe3+The solution concentrations were: 1X 10-2 mol/L、1×10-3mol/L、1×10-4 mol/L、1×10-5 mol/L、1×10-6 mol/L、1×10-7 mol/L；
The detection method comprises the following steps: liquid detection: dropping the solution to be measured to Fe3+The method comprises the following steps of (1) carrying out fluorescence detection on a test strip, or immersing the test strip into solutions to be detected with different concentration gradients, taking out the test strip, and airing the test strip; solid detection: coating the solid powder or particles on a test strip; under the irradiation of 365nm ultraviolet lamp wavelength light, the test paper strip is used for detecting Fe with different concentrations3+The solution presents quenching phenomena of different degrees, thereby realizing the purpose of quenching Fe in sewage3+The qualitative detection of (a) is carried out,
after the detection is finished, soaking the test strip in 100mL of absolute ethyl alcohol for 4min to obtain Fe3+Dissolving the test strip in ethanol, recovering the fluorescence intensity of the test strip, and continuously using the test strip for next detection;
reusable Fe3+The fluorescent test strip is prepared by the following method:
(1) preparing a fluorescent porous material HPP-6:
1mmol of octavinyl silsesquioxane 633mg and 0.4mmol of catalyst Pd (OAc) under the protection of argon290mg, 0.94mmol of cocatalyst P (o-CH)3Ph)3193mg, acid absorbent Et3Dissolving N15mL in 45mL of dry N, N-dimethylformamide, magnetically stirring at room temperature for 0.5h, adding 2mmol of 1.264g of 2,2',7,7' -tetrabromo-9, 9' -spirobifluorene, and reacting at 120 ℃ for 72 h;
and (3) post-treatment: performing suction filtration, washing with tetrahydrofuran, chloroform, water, methanol and acetone respectively, performing Soxhlet extraction with tetrahydrofuran and methanol respectively for 24h, and vacuum drying at 70 ℃ for 48h to obtain yellow solid; the yield is 100%;
(2) preparation of fluorescence detection test strip
Taking a certain amount of the fluorescent porous material HPP-6, uniformly grinding the fluorescent porous material HPP-6 in a mortar, dispersing the ground fluorescent porous material HPP-6 in absolute ethyl alcohol to prepare 40mL of 0.5mg/mL suspension, and ultrasonically dispersing the suspension for 30min to uniformly disperse the suspension; then putting the filter paper into the solution to enable Fe3+The fluorescent material is uniformly deposited on the filter paper, and is taken out and naturally dried; finally, the filter paper is cut into test strips with the length of 5cm and the width of 1 cm.
2. Rapid detection Fe3+The specific method comprises the following steps:
preparing a solution to be detected: preparing Fe with different concentrations3+Solution: fe3+The solution concentrations were: 1X 10-2 mol/L、1×10-3mol/L、1×10-4 mol/L、1×10-5 mol/L、1×10-6 mol/L、1×10-7 mol/L；
The detection method comprises the following steps: mixing Fe3+The fluorescence detection test strip is respectively immersed in Fe with different concentration gradients3+In the solution, after the test strip is dried, the test strip is irradiated by ultraviolet light with the wavelength of 365nm, and the test strip can be used for treating Fe with different concentrations3+The solution presents quenching phenomena of different degrees, thereby realizing the purpose of quenching Fe in sewage3+The qualitative detection of (a) is carried out,
after the detection is finished, soaking the test strip in 100mL of absolute ethyl alcohol for 4min to obtain Fe3+Dissolving the test strip in ethanol, recovering the fluorescence intensity of the test strip, and continuously using the test strip for next detection;
reusable Fe3+The fluorescent test strip is prepared by the following method:
(1) preparing a fluorescent porous material HPP-1:
1mmol of octavinyl silsesquioxane 633mg and 0.4mmol of catalyst Pd (OAc) under the protection of argon290mg, 0.94mmol of cocatalyst P (o-CH)3Ph)3193mg, 16mmol of acid absorbent K2CO32.2g solutionDissolving in 45mL of dry N, N-dimethylformamide, magnetically stirring for 0.5h at room temperature, adding 1.248g of 2mmol of 4,4' -dibromobiphenyl, and reacting for 72h at 120 ℃;
and (3) post-treatment: performing suction filtration, washing with tetrahydrofuran, chloroform, water, methanol and acetone respectively, performing Soxhlet extraction with tetrahydrofuran and methanol respectively for 24h, and vacuum drying at 70 deg.C for 48h to obtain white solid with a yield of 100%;
(2) preparation of fluorescence detection test strip
Taking a certain amount of the fluorescent porous material HPP-1, uniformly grinding in a mortar, dispersing in absolute ethyl alcohol to prepare 40mL of 0.5mg/mL suspension, and ultrasonically dispersing for 30min to uniformly disperse; then putting the filter paper into the solution to enable the fluorescent material to be uniformly deposited on the filter paper, taking out and naturally drying; finally, the filter paper is cut into test strips with the length of 5cm and the width of 1 cm.
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